HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroacetate → Ethyl[3-(4-chlorophenyl)-4-(4-methoxyphenylmethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroacetate | HCID 7751 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-(4-chlorophenyl)-4-(4-methoxybenzyl)-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 58012280 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Ethyl[3-(4-chlorophenyl)-4-(4-methoxyphenylmethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-acetate | HCID 58012215 | — |
Reaction Steps
2.54 g (18.4 mmol) of potassium carbonate are added to 2.90 g (9.18 mmol) of 5-(4-chlorophenyl)-4-(4-methoxyphenylmethyl)-2,4-dihydro-3H-1,2,4-triazol-3-one from Example 55A and 1.13 g (9.18 mmol) of ethyl chloroacetate in 60 ml acetonitrile and the mixture is heated under reflux overnight with stirring. It is then concentrated, the residue is partitioned between ethyl acetate and water and the aqueous phase extracted three times more with ethyl acetate. By evaporation of the organic phases, combined and dried over magnesium sulphate, 3.58 g (97% of theory) of the target compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08084481B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-735cfc622841487a849a9216231a326b |
| Source note | uspto-grants-2011_12 |